Xu Jin-Di, Wu Jie, Zhou Shan-Shan, Shen Hong, Mao Qian, Zhu He, Kong Ming, Li Song-Lin
Department of Pharmaceutical Analysis and Metabolomics, Jiangsu Province Academy of Traditional Chinese Medicine and Jiangsu Branch of China Academy of Chinese Medical Sciences, Nanjing 210028, PR China.
Department of Pharmaceutical Analysis and Metabolomics, Jiangsu Province Academy of Traditional Chinese Medicine and Jiangsu Branch of China Academy of Chinese Medical Sciences, Nanjing 210028, PR China.
J Pharm Biomed Anal. 2015 Aug 10;112:139-46. doi: 10.1016/j.jpba.2015.04.015. Epub 2015 Apr 30.
An improved high performance liquid chromatography-electrospray ionization-mass spectrometry (HPLC-ESI-MS) method was developed to quantitatively evaluate the holistic quality of traditional complex herbal medicines (CHMs). Qiong-Yu-Gao (QYG), a classical CHM consisting of Rehmanniae Radix, Poriae and Ginseng Radix, was used as an example. Thirty-eight major components (including six pairs of epimers/isomers) belonging to five chemical types, i.e., iridoid glycosides, phenethylacohol glycosides, furfural derivatives, ginsenosides and triterpenoid acids, were selected as marker compounds. Programmed ionization mode switching and time segment scanning were designed to improve the sensitivity of the MS detection concerning the diverse chemical features of the analytes. The reference compounds of the analytes were individually injected directly into MS to optimize the ionization cone voltage and to select monitoring ion of each analyte. Nine channels with eight time segments were determined for monitoring the thirty-eight analytes, among which six were detected in positive and thirty-two in negative ion modes respectively. Higher signal-to-noise ratios of the analytes were achieved when compared with full time scanning. In addition, the linearity, precision, accuracy and stability of the method were also validated. The established method was applied for the quantitative evaluation of QYG samples prepared with three different methods. Obvious difference in the contents of thirty-eight components, in particular the original ginsenosides, degraded ginsenosides and furfural derivatives, was found among these QYG samples. All these results demonstrated that the established HPLC-ESI-MS with programmed ionization mode switching and time segment scanning approach is very suitable for the standardization investigation of CHMs.
建立了一种改进的高效液相色谱 - 电喷雾电离 - 质谱（HPLC - ESI - MS）方法，用于定量评估传统复方草药（CHM）的整体质量。以琼玉膏（QYG）为例，它是一种由熟地黄、茯苓和人参组成的经典CHM。选择了属于五种化学类型的38种主要成分（包括六对差向异构体/异构体），即环烯醚萜苷、苯乙醇苷、糠醛衍生物、人参皂苷和三萜酸作为标记化合物。设计了程序电离模式切换和时间段扫描，以提高MS检测对分析物不同化学特征的灵敏度。将分析物的参考化合物分别直接注入MS中，以优化电离锥电压并选择每种分析物的监测离子。确定了九个通道和八个时间段来监测38种分析物，其中六种在正离子模式下检测，32种在负离子模式下检测。与全时扫描相比，分析物的信噪比更高。此外，还验证了该方法的线性、精密度、准确度和稳定性。将所建立的方法应用于用三种不同方法制备的QYG样品的定量评估。在这些QYG样品中，发现38种成分的含量存在明显差异，特别是原人参皂苷、降解人参皂苷和糠醛衍生物。所有这些结果表明，所建立的具有程序电离模式切换和时间段扫描方法的HPLC - ESI - MS非常适合CHM的标准化研究。
